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A method for the oxidation of aromatic beta-diketones to synthesize carboxylic acids

A technology for synthesizing carboxylic acids and aromatics, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., can solve problems such as β-diketones that have not been reported, and achieve short synthesis time and low catalyst consumption The effect of less, high yield

Inactive Publication Date: 2019-02-01
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the use of POMs in the oxidation of β-diketones to carboxylic acids.

Method used

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  • A method for the oxidation of aromatic beta-diketones to synthesize carboxylic acids
  • A method for the oxidation of aromatic beta-diketones to synthesize carboxylic acids
  • A method for the oxidation of aromatic beta-diketones to synthesize carboxylic acids

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] [TEAH] n h 3-n PW 12 o 40 preparation of

[0023] Dissolve 5g of Keggin-type phosphotungstic acid completely in deionized water and stir until dissolved. Then, another n (n=1, 2, 3) times stoichiometric amount of triethylamine was added dropwise to the above solution, and it was observed that a white precipitate would be produced immediately, and the suspension was stirred for 24 hours at room temperature, and then carried out Suction filtration, the filter residue was washed several times with deionized water, and the obtained crude product was dried at 30°C for 12 hours to obtain a white solid product, which was recorded as [TEAH] n h 3-n PW 12 o 40 (eg.TEA:P=1:1 is recorded as [TEAH]H 2 PW 12 o 40 ,TEA:P=2:1 is recorded as [TEAH] 2 HPW 12 o 40 ,TEA:P=3:1 is recorded as [TEAH] 3 PW 12 o 40 ). Phosphotungstic acid and [TEAH] n h 3-n PW 12 o 40 The X-ray powder diffraction pattern is shown in the attached image 3 , indicating that the modification...

Embodiment 2

[0026] The catalyst is [TEAH] 2 HPW 12 o 40(S / C=300), repeat Example 1.

Embodiment 3

[0028] The catalyst is [TEAH] 3 PW 12 o 40 (S / C=300), repeat Example 1. The reaction result is attached figure 1 , indicating that when n(TEA):n(H 3 PW 12 o 40 )=1:1, the prepared catalyst has the best photocatalytic activity.

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Abstract

The invention relates to a method oxidizing aromatic beta-diketone to synthesize carboxylic acid and belongs to the technical field of heterogeneous catalysis organic synthesis. The method specifically includes: under a condition that hydrogen peroxide is used as the oxidizing agent and acetone is used as the solvent, using a heteropoly acid ammonium salt composite photocatalyst [TEAH]nH3-nPW12O40 or [TEAH]nH3-nPW12O40 / SBA-15 to directly photo-catalytically oxidize the aromatic beta-diketone to synthesize the aromatic carboxylic acid. The method is simple, easy to operate, short in synthesizing time, mild in reaction condition (normal temperature and normal pressure) and high in catalyzing efficiency, and especially the selectivity of benzoylacetone can reach up to 97.82%.

Description

technical field [0001] The invention relates to a method for synthesizing carboxylic acid by photocatalytic oxidation of aromatic β-diketone. Specifically, hydrogen peroxide is used as an oxidant, acetone is used as a solvent, and a heteropolyacid ammonium salt composite catalyst is used for photocatalysis under normal temperature and pressure. The invention relates to the synthesis of aromatic carboxylic acid by oxidizing aromatic β-diketone, which belongs to the technical field of organic synthesis. Background technique [0002] Carboxylic acid and its derivatives are a class of chemical raw materials with great industrial value, such as pharmaceuticals, cosmetics, pesticides, food additives and other fields have a very wide range of applications. Therefore, scientists continue to study and explore the synthesis methods of carboxylic acids, among which the oxidation of β-diketones to prepare carboxylic acids has attracted the attention of many chemists. At present, althou...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/285C07C63/06C07C63/04B01J31/18
CPCB01J31/1845B01J2231/70C07C51/285C07C63/06C07C63/04
Inventor 杨平桂成宜赵苏青
Owner EAST CHINA NORMAL UNIV
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